一维NOESY技术在醇胺混合物分析中的应用
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摘要
N-甲基二乙醇胺、三乙醇胺、2-二异丙基氨基乙醇分别属于化武相关化合物氮芥气HN2、氮芥气HN3、神经性毒剂Vx前体化合物。采用一维NOESY选择性激发核磁共振技术实现了高背景干扰下对痕量3种醇胺类化合物相关峰的指认和结构的鉴定。方法对三乙醇胺、N-甲基二乙醇胺、2-二异丙基氨基乙醇检测限(S/N>3)分别为5,10,10μg/m L。该方法简单、快速、不需要复杂的样品前处理步骤,可以有效排除背景干扰,解决核磁共振氢谱中目标化合物部分峰被掩盖,无法对化合物实施充分鉴定的情况。以第32次禁化武组织的水平考试编号322的有机样品为基质,添加20μg/m L 3种醇胺化合物,使用该方法进行分析,取得了良好的效果。
N-methyldiethanolamine,tris( 2-hydroxyethyl) amine,2-( diisopropylamino) ethanol are the precursors of nitrogen mustard HN2,nitrogen mustard HN3,nerve agent Vx respectively. 1 D selective NOESY method was usedsuccessfullyto detect and identify three alcohol amines at trace level with high background. The LODs of this method for the determination of tris( 2-hydroxyethyl) amine,N-methyldiethanolamine,2-( diisopropylamino) ethanol was 5,10 and 10 μg/m L respectively. This method was simple,fast and can wipe off the interference effectively in the ~1H NMR spectrum without complex sample pretreatment. It was useful for the identification of the target chemicals when their peaks were partly covered in ~1H NMR spectrum. These three chemicals at 20 μg/m L were spiked in the organic samplewhich code number was 322 from 32 th OPCW Official Proficiency Tests and were analyzed successfully with this method.
N-methyldiethanolamine,tris( 2-hydroxyethyl) amine,2-( diisopropylamino) ethanol are the precursors of nitrogen mustard HN2,nitrogen mustard HN3,nerve agent Vx respectively. 1 D selective NOESY method was usedsuccessfullyto detect and identify three alcohol amines at trace level with high background. The LODs of this method for the determination of tris( 2-hydroxyethyl) amine,N-methyldiethanolamine,2-( diisopropylamino) ethanol was 5,10 and 10 μg/m L respectively. This method was simple,fast and can wipe off the interference effectively in the ~1H NMR spectrum without complex sample pretreatment. It was useful for the identification of the target chemicals when their peaks were partly covered in ~1H NMR spectrum. These three chemicals at 20 μg/m L were spiked in the organic samplewhich code number was 322 from 32 th OPCW Official Proficiency Tests and were analyzed successfully with this method.
引文
[1]Hu C Y,Lou Y H,Zhou Y X.J Instrum Anal,2001,20(3):81胡绪英,娄艳红,周永新.分析测试学报,2001,20(3):81
[2]Read R W,Black R M.J Anal Toxicol,2004,28(5):346
[3]Zhang L B,Zhang C H,Yu H L,Li X H,Liu J Q.Anal Instrum,2014(3):66张兰波,张春红,于惠兰,李欣海,刘景全.分析仪器,2014,45(3):66
[4]Li J M,Zhang T,Zou N.J Anal Sci,2012,28(4):547李继民,张婷,邹宁.分析科学学报,2012,28(4):547
[5]Zhang H,Huang G L,Yuan L,Li T.Chem Anal Meter,2017,26(3):117张何,黄桂兰,袁铃,李腾.化学分析计量,2017,26(3):117
[6]Liu M K,Guo Q S,Yu S,Xu X.Chinese J Anal Lab,2015,34(11):1343刘明珂,郭强胜,禹珊,许旭.分析实验室,2015,34(11):1343
[7]Deng X J,Li W B,Liu S N,Ding G S.Chin J Anal Lab,2017,36(9):1032邓小娟,李文斌,刘塞纳,丁国生.分析实验室,2017,36(9):1032
[8]Mazumder A,Kumar A,Purohit A K,Dubey D K.Anal Bio Chem,2012,402(4):1643
[9]Huang G L,Yuan L,Liu S L,Zhou S K.Chinese J Anal Chem,2015,43(12):1927黄桂兰,袁铃,刘石磊,周世坤.分析化学,2015,43(12):1927
[10]Liao X J,Zhang X D,Li L Y,Ye C H.Chin J Magn Reson,1997,14(1):69缪希茄,张晓东,李丽云,叶朝辉等.波谱学杂志,1997,14(1):69
[11]Zhao Y,Geng Z F,Deng Z W.Chin J Anal Lab,2016,35(12):1326赵羽,耿珠峰,邓志威.分析实验室,2016,35(12):1326
[12]Lin L,Wei Z,Lin Y,Chen Z.J Magn Reson,2016,272:20
[13]Jeannerat D,Furrer J.Comb Chem High T Scr,2012,15(1):15
[14]Luo Q,Pan Y N,Wei Y,Deng Z W.Mod Instrum,2005,11(2):10罗权,潘燕娜,韦轶,邓志威.现代仪器,2005,11(2):10
[15]Zhou Y L,Li H L.Chin J Org Chem,1986,1(1):3周原朗,李华立.有机化学,1986,1(1):3
[16]Ning Y C.Structural Identification of Organic Compounds and Organic spectroscopy(Second Edition).Beijing:Science Press,2000:199宁永成.有机化合物结构鉴定与有机波谱学(第2版).北京:科学出版社,2000:199
[17]Mao X A.Practical technology and application of modern nuclear magnetic resonance.Beijing:Science and Technology Literature Press,2000:135毛希安.现代核磁共振实用技术及应用.北京:科学技术文献出版社,2000:135
[18]Timothy D W Claridge.High-Resolution NMR Techniques in Origanic Chemistry.Oxford:Pergamon Press,2009:236
[19]Lundstr9m P.Nuclear Overhauser Effect.Berlin:Springer,2013:197
[2]Read R W,Black R M.J Anal Toxicol,2004,28(5):346
[3]Zhang L B,Zhang C H,Yu H L,Li X H,Liu J Q.Anal Instrum,2014(3):66张兰波,张春红,于惠兰,李欣海,刘景全.分析仪器,2014,45(3):66
[4]Li J M,Zhang T,Zou N.J Anal Sci,2012,28(4):547李继民,张婷,邹宁.分析科学学报,2012,28(4):547
[5]Zhang H,Huang G L,Yuan L,Li T.Chem Anal Meter,2017,26(3):117张何,黄桂兰,袁铃,李腾.化学分析计量,2017,26(3):117
[6]Liu M K,Guo Q S,Yu S,Xu X.Chinese J Anal Lab,2015,34(11):1343刘明珂,郭强胜,禹珊,许旭.分析实验室,2015,34(11):1343
[7]Deng X J,Li W B,Liu S N,Ding G S.Chin J Anal Lab,2017,36(9):1032邓小娟,李文斌,刘塞纳,丁国生.分析实验室,2017,36(9):1032
[8]Mazumder A,Kumar A,Purohit A K,Dubey D K.Anal Bio Chem,2012,402(4):1643
[9]Huang G L,Yuan L,Liu S L,Zhou S K.Chinese J Anal Chem,2015,43(12):1927黄桂兰,袁铃,刘石磊,周世坤.分析化学,2015,43(12):1927
[10]Liao X J,Zhang X D,Li L Y,Ye C H.Chin J Magn Reson,1997,14(1):69缪希茄,张晓东,李丽云,叶朝辉等.波谱学杂志,1997,14(1):69
[11]Zhao Y,Geng Z F,Deng Z W.Chin J Anal Lab,2016,35(12):1326赵羽,耿珠峰,邓志威.分析实验室,2016,35(12):1326
[12]Lin L,Wei Z,Lin Y,Chen Z.J Magn Reson,2016,272:20
[13]Jeannerat D,Furrer J.Comb Chem High T Scr,2012,15(1):15
[14]Luo Q,Pan Y N,Wei Y,Deng Z W.Mod Instrum,2005,11(2):10罗权,潘燕娜,韦轶,邓志威.现代仪器,2005,11(2):10
[15]Zhou Y L,Li H L.Chin J Org Chem,1986,1(1):3周原朗,李华立.有机化学,1986,1(1):3
[16]Ning Y C.Structural Identification of Organic Compounds and Organic spectroscopy(Second Edition).Beijing:Science Press,2000:199宁永成.有机化合物结构鉴定与有机波谱学(第2版).北京:科学出版社,2000:199
[17]Mao X A.Practical technology and application of modern nuclear magnetic resonance.Beijing:Science and Technology Literature Press,2000:135毛希安.现代核磁共振实用技术及应用.北京:科学技术文献出版社,2000:135
[18]Timothy D W Claridge.High-Resolution NMR Techniques in Origanic Chemistry.Oxford:Pergamon Press,2009:236
[19]Lundstr9m P.Nuclear Overhauser Effect.Berlin:Springer,2013:197